A polysaccharide from V. cholera extracted by two methods was analyzed for monosaccharide composition by preparing the TMS derivatives of the methylglycosides followed by combined GC/MS analysis. TMS methylglycosides were prepared from the samples by methanolysis in 1 M HCl in methanol, followed by N-acetylation with pyridine and acetic anhydride. The samples were then treated with Tri-Sil. GC/MS analysis of the TMS methylglycosides was performed using a Hewlett Packard 5890 GC coupled to a 5970 MSD using a DB1 fused capillary column. Monosaccharides were identified by their retention times in comparison to standards, and their carbohydrate character was authenticated by their mass spectra.